Kamran Abro - Academia.edu (original) (raw)

Papers by Kamran Abro

Research paper thumbnail of FTIR characterization and physicochemical evaluation of cottonseed oil

Pakistan Journal of Analytical & Environmental Chemistry, 2017

In present study, cottonseed (Gossypium) varieties (RH-112, Lankart-57, K-25, F-20 and D-9) were ... more In present study, cottonseed (Gossypium) varieties (RH-112, Lankart-57, K-25, F-20 and D-9) were evaluated for possible variation in quality attributes by using conventional and instrumental techniques. Physiochemical characteristics of seed and oils varied as: weight of individual seed (0.069-0.085 g), weight of 100 seeds (5.95-7.73 g), width (0.461-0.544 cm), length (0.736-0.915 cm), moisture (6.2-8.5%), oil content (12.01 to14.55%), refractive index at 40 o C (1.4661-1.4665) iodine value (IV) (93.90-105.76 gI 2 /100g), saponification value (SV) (181.83-190.55 mg KOH/g), peroxide value (PV) (1.0-6.0 m Eq/Kg), free fatty acids (FFA) (17.30-38.80 %) and induction period (IP) (1.95-2.65 h), respectively. Analyzed varieties showed higher level of FFA (17.30-38.80%), while lower level of IP (1.95-2.65 h) respectively. Furthermore, GC-FID and FT-IR studies were carried out for quantitative and qualitative analysis of cottonseed oil. Analysis showed that most abundant fatty acid in each variety was linoleic acid (42.09-52.55 %) among unsaturated fatty acids, whereas palmitic acid (22.70-26.20 %) was major saturated fatty acid. Some band intensities of FTIR spectra highly correlated with the chemical properties of cottonseed oil such as IV, SV, PV, FFA and IP. In conclusion significant variation in physiochemical properties was observed among five cottonseed varieties, especially FFA and IP of cottonseed oil which is not good for the quality and edible point of view. This can be associated with the specific genetic variability and climatic conditions.

Research paper thumbnail of Simpler and Faster Spectrophotometric Determination of Diclofenac Sodium in Tablets, Serum and Urine Samples

This work describes a simple, sensitive, rapid and economical analytical procedure for direct spe... more This work describes a simple, sensitive, rapid and economical analytical procedure for direct spectrophotometric evaluation of diclofenac sodium (DS) using aqueous medium without using a chemical reagent. Parameters like time, temperature, acidic and basic conditions and interference by analgesic drugs were studied for a 5µg ml-1 solution of DS at 276 nm. Under optimized parameters, a linear working range of 0.1-30 µg ml-1 with regression coefficient of 0.9998 and lower detection limit of 0.01 µg ml-1 was obtained. The method was applied for DS contents in tablets, serum and urine samples.

Research paper thumbnail of Efficacy Studies of Two Iron Supplements Irovit-1 and Irovit-2

Pakistan Journal of Scientific & Industrial Research Series A: Physical Sciences, 2021

Two preparations of iron supplements have been developed with vitamins, Irovit-1 and Irovit-2 con... more Two preparations of iron supplements have been developed with vitamins, Irovit-1 and Irovit-2 containing 1 mg/mL and 2 mg/mL elemental iron respectively in complex form. Clinical trials of Irovit-1 and Irovit-2 have been conducted randomly on selected anemic males and females from urban population of Karachi, an improvement in hemoglobin levels were estimated for the treatments with Irovit-1 (10 mg Fe/day) and Irovit-2 (20 mg Fe/day). Both preparations have been found to be effective in increasing hemoglobin, Hematocrit and red blood cell count. The mean hemoglobin levels were observed increased 0.73 ± 0.25 g/dL and 1.10 ± 0.30 g/dL, after 5 weeks by oral intake of Irovit-1 and Irovit-2, respectively.

Research paper thumbnail of HPLC Determination of Betamethasone and Prednisolone in Urine Samples Using Monolithic Column

Pakistan Journal of Scientific & Industrial Research Series A: Physical Sciences, 2011

Research paper thumbnail of Sequential Microwave-Assisted Extraction of Oil from Layer Poultry Feeds and GC-MS Quantification of the Fatty Acids

The present study reports the effect of sequential microwave-assisted extraction (SeMAE) on fatty... more The present study reports the effect of sequential microwave-assisted extraction (SeMAE) on fatty acids composition (FAC) of layer poultry feed oil as compared to conventional Soxhlet extraction (SE) method. The FAC of extracted oil was determined by gas chromatography-mass spectrometry (GC-MS). There was no significant difference found in the amount of total extracted oil and FAC by SeMAE and SE. However, slightly greater content of trans fat in the samples revealed that SE lead to the formation of a little higher level of trans fat as compare to SeMAE. Therefore, the SeMAE could be used as a remarkable substitute to conventional SE for extraction of oil from the poultry feeds due to its faster speed, lesser solvent consumption, more environmental friendly.

Research paper thumbnail of Recent Progress in the Analysis of Captopril Using Electrochemical Methods: A Review

Current Analytical Chemistry, 2019

Background: Captopril is the synthetic dipeptide used as an angiotensin converting enzyme inhibit... more Background: Captopril is the synthetic dipeptide used as an angiotensin converting enzyme inhibitor. Captopril is used to treat hypertension as well as for the treatment of moderate heart failure. Analytical instrumentation and methodology plays an important role in pharmaceutical analysis. Methods: This review presents some important applications of electrochemical modes used for the analysis of captopril. So far captopril has been analyzed by using different bare and modified working electrodes with a variety of modifiers from organic and inorganic materials to various types of nano particles/materials. Results: This paper presents some of the methods which have been published in the last few years i.e. from 2003 to 2016. This review highlights the role of the analytical instrumentation, particularly electrochemical methods in assessing captopril using various working electrodes. Conclusion: A large number of studies on voltammetry noted by means of various bare and modified elect...

Research paper thumbnail of GC-MS Evaluation of Fatty Acid Profile and Lipid Bioactive of Partially Hydrogenated Cooking Oil Consumed in Pakistan

Pakistan journal of scientific and industrial research

Research paper thumbnail of Determination of Vitamin E-Acetate, D3, and K1 in Plasma Samples by Liquid Chromatography-Atmospheric Pressure Chemical Ionization- Mass Spectrometry Utilizing a Monolithic Column

Analytical Letters

The purpose of this study was to develop a rapid, simple and sensitive method for simultaneous de... more The purpose of this study was to develop a rapid, simple and sensitive method for simultaneous determination of Vitamin-D3 (vitamin-D3), Vitamin E-Acetate (vitamin-EA) and Vitamin-K-1 (vitamin-K1) in plasma using LC-APCI-MS with monolithic column as stationary phase. Plasma samples were cleaned up using solid phase extraction. The separation of compounds were achieved using monolithic column (C-18) and mobile phase composed of methanol and 0.1% formic acid in gradient elution mode at the flow rate of 1.0 mL min-1. Analytes were ionized using atmospheric chemical ionization in positive mode. Mass spectra were recorded at 385.23, 473.47 and 451.41 m/z for vitamin-D3, vitamin-EA and vitamin-K1 respectively whereas vitamin-D2 (vitamin-D2) was used as an internal standard (IS) and its mass spectra was recorded at 397.28 m/z. The method is validated using ICH guidelines. The system suitability response were calculated for reproducibility tests of the retention time, number of theoretical ...

Research paper thumbnail of Application of microwave heating for the fast extraction of fat content from the poultry feeds

Talanta, 2008

A rapid method has been developed to extract and quantitatively measure the total oil content in ... more A rapid method has been developed to extract and quantitatively measure the total oil content in poultry feeds using a domestic microwave oven. The optimized extraction procedure involves the replicate (6×) extraction of 5 g of ground feed with 12 ml of hexane for 20 s in a 900 W oven. Each replicate involves the collection of the resulting miscella and its replacement with fresh solvent for re-extraction. The collected extracts were centrifuged and transferred to a vial. The solvent was evaporated to a constant weight and the residual lipid weighed. In comparison to conventional Soxhlet extraction method, lipid contents obtained using the optimized microwave procedure was not significantly different. However, FTIR analysis indicated that the microwave procedure was superior in minimizing the formation of free fatty acids (FFA) relative to the Soxhlet procedure if the temperature of the sample was kept within the range of 45-50 • C. This simple, sequential extraction procedure is rapid, highly efficient and provides a simple mean of quantitating the lipid content of poultry feed in less than 40 min without the need for specialized microwave oven.

Research paper thumbnail of Multi-component quantitation of loratadine, pseudoephedrine and paracetamol in plasma and pharmaceutical formulations with liquid chromatography-tandem mass spectrometry utilizing a monolithic column

Química Nova, 2012

The purpose of this study was to develop a rapid, simple and sensitive quantitation method for ps... more The purpose of this study was to develop a rapid, simple and sensitive quantitation method for pseudoephedrine (PSE), paracetamol (PAR) and loratadine (LOR) in plasma and pharmaceuticals using liquid chromatography-tandem mass spectrometry with a monolithic column. Separation was achieved using a gradient composition of methanol-0.1% formic acid at a flow rate of 1.0 mL min-1. Mass spectral transitions were recorded in SRM mode. System validation was evaluated for precision, specificity and linearity. Limit of detection for pseudoephedrine, paracetamol, and loratadine were determined to be 3.14, 1.86 and 1.44 ng mL-1 , respectively, allowing easy determination in plasma with % recovery of 93.12 to 101.56%.

Research paper thumbnail of Quantification of malachite green in fish feed utilising liquid chromatography-tandem mass spectrometry with a monolithic column

Food Additives & Contaminants: Part A, 2014

The purpose of this study was to develop a rapid and sensitive method for the quantification of m... more The purpose of this study was to develop a rapid and sensitive method for the quantification of malachite green (MG) in fish feed using LC-ESI-MS/MS with a monolithic column as stationary phase. Fish feed was cleaned using ultrasonic assisted liquid-liquid extraction. The separation was achieved on a Chromolith® Performance RP-18e column (100 × 4.6 mm) using gradient mobile phase composition of methanol and 0.1% formic acid at the flow rate of 1.0 ml min⁻¹. The analyte was ionised using electrospray ionisation in positive mode. Mass spectral transitions were recorded in selected reaction monitoring (SRM) mode at m/z 329.78 → m/z 314.75 with a collision energy (CE) of 52% for MG. The system suitability responses were calculated for reproducibility tests of the retention time, number of theoretical plates and capacity factor. System validation was evaluated for precision, specificity and linearity of MG. The linearity and calibration graph was plotted in the range of 15.0-250 ng ml⁻¹ with the regression coefficient of >0.997. The lower limits of detection and quantification for MG were 0.55 and 1.44 ng ml⁻¹, respectively, allowing easy determination in fish feed with accuracy evaluated as a percentage recovery of 92.1% and precision determined as % CV of < 5. The method was also extended to the determination of MG in an actual fish feed. The sensitivity and selectivity of LC-ESI-MS/MS using monolithic column offers a valuable alternative to the methodologies currently employed for the quantification of MG in fish feeds.

Research paper thumbnail of Determination of Vitamins E, D3, and K1 in Plasma by Liquid Chromatography-Atmospheric Pressure Chemical Ionization-Mass Spectrometry Utilizing a Monolithic Column

Analytical Letters, 2013

ABSTRACT This paper reports a rapid, simple, and sensitive method for determination of vitamin D3... more ABSTRACT This paper reports a rapid, simple, and sensitive method for determination of vitamin D3, vitamin E acetate, and vitamin K1 in plasma using atmospheric pressure chemical ionization –high performance liquid chromatography–mass spectrometry. Plasma samples were prepared using solid phase extraction. The separation of compounds was achieved using a C18 monolithic column and a mobile phase composed of methanol and 0.1% formic acid in gradient elution mode at a flow rate of 1.0 mL min−1. Analytes were ionized using atmospheric chemical ionization in positive mode. Mass spectra were recorded at m/z = 385.23, 473.47, and 451.41 for vitamin D3, vitamin E, and vitamin K1, respectively. Vitamin D2 was used as an internal standard and its mass spectra was recorded at 397.28 m/z. The method was validated using ICH guidelines. The system suitability responses were calculated for retention time, number of theoretical plates, capacity factor, resolution, and the selectivity factor. System validation was evaluated for precision, specificity, and linearity of all compounds. The limits of detection for vitamin D3, vitamin E, and vitamin K1 were determined to be 0.1, 1.36, and 0.052 ng mL−1, respectively. The accuracy, evaluated as % of recovery, was in the range of 96.4 to 102.4% and precision determined as the coefficient of variation was between 1.24 and 3.6%. The validated method was applied to real plasma samples.

Research paper thumbnail of Comparative Study of Electrospray and Atmospheric Pressure Chemical Ionization with Liquid Chromatography–Mass Spectrometry for Quantification of Five Antihyperglycemic Agents Utilizing Monolithic Column

Analytical Letters, 2012

Liquid chromatography-mass spectrometry (LC-MS) in atmospheric pressure chemical ionization (APCI... more Liquid chromatography-mass spectrometry (LC-MS) in atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI) modes were studied for a multi-component plasma and urine quantification of 5 antihyperglycemic agents (metformin, pioglitazone, gliclazide, glibenclamide and glimperide). The separation of the compounds was achieved using Chromolith® Performance RP-18e column (100 × 4.6 mm), with gradient mobile phase composition of acetonitrile-0.1% formic acid. MS parameters for APCI

Research paper thumbnail of Liquid Chromatographic Determination of Pioglitazone in Pharmaceuticals, Serum and Urine Samples

Pakistan Journal of Analytical and Environmental Chemistry, 2011

A rapid and reliable analytical method based on high-performance liquid chromatography (HPLC) wit... more A rapid and reliable analytical method based on high-performance liquid chromatography (HPLC) with UV detection (221nm) has been developed for the determination of the anti-hyperglycemic agent Pioglitazone in pharmaceutical formulations and biological fluids (serum and urine) after clean-up with solid-phase extraction. Chromatographic separation was achieved with a Chromolith

Research paper thumbnail of LC/UV determination of cefradine, cefuroxime, and cefotaxime in dairy milk, human serum and wastewater samples

SpringerPlus, 2013

Cephalosporins type antibiotics are widely used to treat infectious diseases. Their determination... more Cephalosporins type antibiotics are widely used to treat infectious diseases. Their determination is not only important in blood/serum of patients under treatment but also in diverse matrices like wastewaters, milk etc. as contaminant. Keeping in view the need, a new high performance liquid chromatographic method for the determination of three cephalosporins (cefradine, cefuroxime and cefotaxime) has been developed. Separation was performed on an ODS column with binary solvent elution of aqueous formic acid (0.05%) and methanol in the ratio of 45: 55 (v/v) at a flow rate of 1 mL min-1 and UV detection at 260 nm. Under optimised conditions, all three cephalosporins were baseline separated within 5 min. Linear responses for cefradine 5–20 μg mL-1, cefuroxime 0.5-15 μg mL-1 and cefotaxime 1.0-20 μg mL-1 were established. LOD of 0.05-0.25 μg mL-1 after preconcentration was achieved. The method was applied to serum samples of patients under treatment with these antibiotics and to screen ...

Research paper thumbnail of FTIR characterization and physicochemical evaluation of cottonseed oil

Pakistan Journal of Analytical & Environmental Chemistry, 2017

In present study, cottonseed (Gossypium) varieties (RH-112, Lankart-57, K-25, F-20 and D-9) were ... more In present study, cottonseed (Gossypium) varieties (RH-112, Lankart-57, K-25, F-20 and D-9) were evaluated for possible variation in quality attributes by using conventional and instrumental techniques. Physiochemical characteristics of seed and oils varied as: weight of individual seed (0.069-0.085 g), weight of 100 seeds (5.95-7.73 g), width (0.461-0.544 cm), length (0.736-0.915 cm), moisture (6.2-8.5%), oil content (12.01 to14.55%), refractive index at 40 o C (1.4661-1.4665) iodine value (IV) (93.90-105.76 gI 2 /100g), saponification value (SV) (181.83-190.55 mg KOH/g), peroxide value (PV) (1.0-6.0 m Eq/Kg), free fatty acids (FFA) (17.30-38.80 %) and induction period (IP) (1.95-2.65 h), respectively. Analyzed varieties showed higher level of FFA (17.30-38.80%), while lower level of IP (1.95-2.65 h) respectively. Furthermore, GC-FID and FT-IR studies were carried out for quantitative and qualitative analysis of cottonseed oil. Analysis showed that most abundant fatty acid in each variety was linoleic acid (42.09-52.55 %) among unsaturated fatty acids, whereas palmitic acid (22.70-26.20 %) was major saturated fatty acid. Some band intensities of FTIR spectra highly correlated with the chemical properties of cottonseed oil such as IV, SV, PV, FFA and IP. In conclusion significant variation in physiochemical properties was observed among five cottonseed varieties, especially FFA and IP of cottonseed oil which is not good for the quality and edible point of view. This can be associated with the specific genetic variability and climatic conditions.

Research paper thumbnail of Simpler and Faster Spectrophotometric Determination of Diclofenac Sodium in Tablets, Serum and Urine Samples

This work describes a simple, sensitive, rapid and economical analytical procedure for direct spe... more This work describes a simple, sensitive, rapid and economical analytical procedure for direct spectrophotometric evaluation of diclofenac sodium (DS) using aqueous medium without using a chemical reagent. Parameters like time, temperature, acidic and basic conditions and interference by analgesic drugs were studied for a 5µg ml-1 solution of DS at 276 nm. Under optimized parameters, a linear working range of 0.1-30 µg ml-1 with regression coefficient of 0.9998 and lower detection limit of 0.01 µg ml-1 was obtained. The method was applied for DS contents in tablets, serum and urine samples.

Research paper thumbnail of Efficacy Studies of Two Iron Supplements Irovit-1 and Irovit-2

Pakistan Journal of Scientific & Industrial Research Series A: Physical Sciences, 2021

Two preparations of iron supplements have been developed with vitamins, Irovit-1 and Irovit-2 con... more Two preparations of iron supplements have been developed with vitamins, Irovit-1 and Irovit-2 containing 1 mg/mL and 2 mg/mL elemental iron respectively in complex form. Clinical trials of Irovit-1 and Irovit-2 have been conducted randomly on selected anemic males and females from urban population of Karachi, an improvement in hemoglobin levels were estimated for the treatments with Irovit-1 (10 mg Fe/day) and Irovit-2 (20 mg Fe/day). Both preparations have been found to be effective in increasing hemoglobin, Hematocrit and red blood cell count. The mean hemoglobin levels were observed increased 0.73 ± 0.25 g/dL and 1.10 ± 0.30 g/dL, after 5 weeks by oral intake of Irovit-1 and Irovit-2, respectively.

Research paper thumbnail of HPLC Determination of Betamethasone and Prednisolone in Urine Samples Using Monolithic Column

Pakistan Journal of Scientific & Industrial Research Series A: Physical Sciences, 2011

Research paper thumbnail of Sequential Microwave-Assisted Extraction of Oil from Layer Poultry Feeds and GC-MS Quantification of the Fatty Acids

The present study reports the effect of sequential microwave-assisted extraction (SeMAE) on fatty... more The present study reports the effect of sequential microwave-assisted extraction (SeMAE) on fatty acids composition (FAC) of layer poultry feed oil as compared to conventional Soxhlet extraction (SE) method. The FAC of extracted oil was determined by gas chromatography-mass spectrometry (GC-MS). There was no significant difference found in the amount of total extracted oil and FAC by SeMAE and SE. However, slightly greater content of trans fat in the samples revealed that SE lead to the formation of a little higher level of trans fat as compare to SeMAE. Therefore, the SeMAE could be used as a remarkable substitute to conventional SE for extraction of oil from the poultry feeds due to its faster speed, lesser solvent consumption, more environmental friendly.

Research paper thumbnail of Recent Progress in the Analysis of Captopril Using Electrochemical Methods: A Review

Current Analytical Chemistry, 2019

Background: Captopril is the synthetic dipeptide used as an angiotensin converting enzyme inhibit... more Background: Captopril is the synthetic dipeptide used as an angiotensin converting enzyme inhibitor. Captopril is used to treat hypertension as well as for the treatment of moderate heart failure. Analytical instrumentation and methodology plays an important role in pharmaceutical analysis. Methods: This review presents some important applications of electrochemical modes used for the analysis of captopril. So far captopril has been analyzed by using different bare and modified working electrodes with a variety of modifiers from organic and inorganic materials to various types of nano particles/materials. Results: This paper presents some of the methods which have been published in the last few years i.e. from 2003 to 2016. This review highlights the role of the analytical instrumentation, particularly electrochemical methods in assessing captopril using various working electrodes. Conclusion: A large number of studies on voltammetry noted by means of various bare and modified elect...

Research paper thumbnail of GC-MS Evaluation of Fatty Acid Profile and Lipid Bioactive of Partially Hydrogenated Cooking Oil Consumed in Pakistan

Pakistan journal of scientific and industrial research

Research paper thumbnail of Determination of Vitamin E-Acetate, D3, and K1 in Plasma Samples by Liquid Chromatography-Atmospheric Pressure Chemical Ionization- Mass Spectrometry Utilizing a Monolithic Column

Analytical Letters

The purpose of this study was to develop a rapid, simple and sensitive method for simultaneous de... more The purpose of this study was to develop a rapid, simple and sensitive method for simultaneous determination of Vitamin-D3 (vitamin-D3), Vitamin E-Acetate (vitamin-EA) and Vitamin-K-1 (vitamin-K1) in plasma using LC-APCI-MS with monolithic column as stationary phase. Plasma samples were cleaned up using solid phase extraction. The separation of compounds were achieved using monolithic column (C-18) and mobile phase composed of methanol and 0.1% formic acid in gradient elution mode at the flow rate of 1.0 mL min-1. Analytes were ionized using atmospheric chemical ionization in positive mode. Mass spectra were recorded at 385.23, 473.47 and 451.41 m/z for vitamin-D3, vitamin-EA and vitamin-K1 respectively whereas vitamin-D2 (vitamin-D2) was used as an internal standard (IS) and its mass spectra was recorded at 397.28 m/z. The method is validated using ICH guidelines. The system suitability response were calculated for reproducibility tests of the retention time, number of theoretical ...

Research paper thumbnail of Application of microwave heating for the fast extraction of fat content from the poultry feeds

Talanta, 2008

A rapid method has been developed to extract and quantitatively measure the total oil content in ... more A rapid method has been developed to extract and quantitatively measure the total oil content in poultry feeds using a domestic microwave oven. The optimized extraction procedure involves the replicate (6×) extraction of 5 g of ground feed with 12 ml of hexane for 20 s in a 900 W oven. Each replicate involves the collection of the resulting miscella and its replacement with fresh solvent for re-extraction. The collected extracts were centrifuged and transferred to a vial. The solvent was evaporated to a constant weight and the residual lipid weighed. In comparison to conventional Soxhlet extraction method, lipid contents obtained using the optimized microwave procedure was not significantly different. However, FTIR analysis indicated that the microwave procedure was superior in minimizing the formation of free fatty acids (FFA) relative to the Soxhlet procedure if the temperature of the sample was kept within the range of 45-50 • C. This simple, sequential extraction procedure is rapid, highly efficient and provides a simple mean of quantitating the lipid content of poultry feed in less than 40 min without the need for specialized microwave oven.

Research paper thumbnail of Multi-component quantitation of loratadine, pseudoephedrine and paracetamol in plasma and pharmaceutical formulations with liquid chromatography-tandem mass spectrometry utilizing a monolithic column

Química Nova, 2012

The purpose of this study was to develop a rapid, simple and sensitive quantitation method for ps... more The purpose of this study was to develop a rapid, simple and sensitive quantitation method for pseudoephedrine (PSE), paracetamol (PAR) and loratadine (LOR) in plasma and pharmaceuticals using liquid chromatography-tandem mass spectrometry with a monolithic column. Separation was achieved using a gradient composition of methanol-0.1% formic acid at a flow rate of 1.0 mL min-1. Mass spectral transitions were recorded in SRM mode. System validation was evaluated for precision, specificity and linearity. Limit of detection for pseudoephedrine, paracetamol, and loratadine were determined to be 3.14, 1.86 and 1.44 ng mL-1 , respectively, allowing easy determination in plasma with % recovery of 93.12 to 101.56%.

Research paper thumbnail of Quantification of malachite green in fish feed utilising liquid chromatography-tandem mass spectrometry with a monolithic column

Food Additives & Contaminants: Part A, 2014

The purpose of this study was to develop a rapid and sensitive method for the quantification of m... more The purpose of this study was to develop a rapid and sensitive method for the quantification of malachite green (MG) in fish feed using LC-ESI-MS/MS with a monolithic column as stationary phase. Fish feed was cleaned using ultrasonic assisted liquid-liquid extraction. The separation was achieved on a Chromolith® Performance RP-18e column (100 × 4.6 mm) using gradient mobile phase composition of methanol and 0.1% formic acid at the flow rate of 1.0 ml min⁻¹. The analyte was ionised using electrospray ionisation in positive mode. Mass spectral transitions were recorded in selected reaction monitoring (SRM) mode at m/z 329.78 → m/z 314.75 with a collision energy (CE) of 52% for MG. The system suitability responses were calculated for reproducibility tests of the retention time, number of theoretical plates and capacity factor. System validation was evaluated for precision, specificity and linearity of MG. The linearity and calibration graph was plotted in the range of 15.0-250 ng ml⁻¹ with the regression coefficient of >0.997. The lower limits of detection and quantification for MG were 0.55 and 1.44 ng ml⁻¹, respectively, allowing easy determination in fish feed with accuracy evaluated as a percentage recovery of 92.1% and precision determined as % CV of < 5. The method was also extended to the determination of MG in an actual fish feed. The sensitivity and selectivity of LC-ESI-MS/MS using monolithic column offers a valuable alternative to the methodologies currently employed for the quantification of MG in fish feeds.

Research paper thumbnail of Determination of Vitamins E, D3, and K1 in Plasma by Liquid Chromatography-Atmospheric Pressure Chemical Ionization-Mass Spectrometry Utilizing a Monolithic Column

Analytical Letters, 2013

ABSTRACT This paper reports a rapid, simple, and sensitive method for determination of vitamin D3... more ABSTRACT This paper reports a rapid, simple, and sensitive method for determination of vitamin D3, vitamin E acetate, and vitamin K1 in plasma using atmospheric pressure chemical ionization –high performance liquid chromatography–mass spectrometry. Plasma samples were prepared using solid phase extraction. The separation of compounds was achieved using a C18 monolithic column and a mobile phase composed of methanol and 0.1% formic acid in gradient elution mode at a flow rate of 1.0 mL min−1. Analytes were ionized using atmospheric chemical ionization in positive mode. Mass spectra were recorded at m/z = 385.23, 473.47, and 451.41 for vitamin D3, vitamin E, and vitamin K1, respectively. Vitamin D2 was used as an internal standard and its mass spectra was recorded at 397.28 m/z. The method was validated using ICH guidelines. The system suitability responses were calculated for retention time, number of theoretical plates, capacity factor, resolution, and the selectivity factor. System validation was evaluated for precision, specificity, and linearity of all compounds. The limits of detection for vitamin D3, vitamin E, and vitamin K1 were determined to be 0.1, 1.36, and 0.052 ng mL−1, respectively. The accuracy, evaluated as % of recovery, was in the range of 96.4 to 102.4% and precision determined as the coefficient of variation was between 1.24 and 3.6%. The validated method was applied to real plasma samples.

Research paper thumbnail of Comparative Study of Electrospray and Atmospheric Pressure Chemical Ionization with Liquid Chromatography–Mass Spectrometry for Quantification of Five Antihyperglycemic Agents Utilizing Monolithic Column

Analytical Letters, 2012

Liquid chromatography-mass spectrometry (LC-MS) in atmospheric pressure chemical ionization (APCI... more Liquid chromatography-mass spectrometry (LC-MS) in atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI) modes were studied for a multi-component plasma and urine quantification of 5 antihyperglycemic agents (metformin, pioglitazone, gliclazide, glibenclamide and glimperide). The separation of the compounds was achieved using Chromolith® Performance RP-18e column (100 × 4.6 mm), with gradient mobile phase composition of acetonitrile-0.1% formic acid. MS parameters for APCI

Research paper thumbnail of Liquid Chromatographic Determination of Pioglitazone in Pharmaceuticals, Serum and Urine Samples

Pakistan Journal of Analytical and Environmental Chemistry, 2011

A rapid and reliable analytical method based on high-performance liquid chromatography (HPLC) wit... more A rapid and reliable analytical method based on high-performance liquid chromatography (HPLC) with UV detection (221nm) has been developed for the determination of the anti-hyperglycemic agent Pioglitazone in pharmaceutical formulations and biological fluids (serum and urine) after clean-up with solid-phase extraction. Chromatographic separation was achieved with a Chromolith

Research paper thumbnail of LC/UV determination of cefradine, cefuroxime, and cefotaxime in dairy milk, human serum and wastewater samples

SpringerPlus, 2013

Cephalosporins type antibiotics are widely used to treat infectious diseases. Their determination... more Cephalosporins type antibiotics are widely used to treat infectious diseases. Their determination is not only important in blood/serum of patients under treatment but also in diverse matrices like wastewaters, milk etc. as contaminant. Keeping in view the need, a new high performance liquid chromatographic method for the determination of three cephalosporins (cefradine, cefuroxime and cefotaxime) has been developed. Separation was performed on an ODS column with binary solvent elution of aqueous formic acid (0.05%) and methanol in the ratio of 45: 55 (v/v) at a flow rate of 1 mL min-1 and UV detection at 260 nm. Under optimised conditions, all three cephalosporins were baseline separated within 5 min. Linear responses for cefradine 5–20 μg mL-1, cefuroxime 0.5-15 μg mL-1 and cefotaxime 1.0-20 μg mL-1 were established. LOD of 0.05-0.25 μg mL-1 after preconcentration was achieved. The method was applied to serum samples of patients under treatment with these antibiotics and to screen ...